JP2010070609A - Easily re-pastable adhesive tape - Google Patents
Easily re-pastable adhesive tape Download PDFInfo
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- JP2010070609A JP2010070609A JP2008237937A JP2008237937A JP2010070609A JP 2010070609 A JP2010070609 A JP 2010070609A JP 2008237937 A JP2008237937 A JP 2008237937A JP 2008237937 A JP2008237937 A JP 2008237937A JP 2010070609 A JP2010070609 A JP 2010070609A
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Abstract
Description
本発明は、貼着不良が発生した際に容易に剥離して貼り直すことが可能な粘着テープに関する。 The present invention relates to an adhesive tape that can be easily peeled off and reattached when a sticking failure occurs.
基材の片面又は両面に粘着剤層が積層された粘着テープは、現在では多種多様な分野に用いられており、あらゆる産業に必須のものとなっている。このような粘着テープの問題点の一つとして、被着体に貼着する際に誤って粘着テープが撚れてしまう等の貼着不良が生じたときに、粘着フィルムを剥離して貼り直すのが困難な場合があるということがある。 Adhesive tapes in which an adhesive layer is laminated on one or both sides of a substrate are currently used in a wide variety of fields, and are indispensable for all industries. One of the problems with such adhesive tapes is that when an adhesive failure occurs, such as when the adhesive tape is accidentally twisted when it is attached to an adherend, the adhesive film is peeled off and reattached. Sometimes it is difficult.
例えば、半導体ウエハをダイシングして個々の半導体チップを製造する工程においては、半導体ウエハの破損等を保護する目的で、ダイシングテープと呼ばれる粘着テープを半導体ウエハに貼着することが行われている（例えば、特許文献１）。ダイシングテープを半導体ウエハに貼着する工程では、通常、空気噛み等が生じないように減圧化で貼着が行われることが多いが、この際に誤ってダイシングテープが撚れてしまう等の貼着不良が発生することがある。このようにダイシングテープが撚れて貼着された状態でダイシングを行うと、正確なダイシングを行うことが困難であるばかりでなく、半導体ウエハを破損してしまうこともある。従って、撚れてしまったダイシングテープを半導体ウエハから剥離して、貼り直すことが望まれる。しかしながら、ダイシングテープを剥離しようとするとする際に、半導体ウエハが破損してしまうことがある。とりわけ、半導体ウエハの厚さが５０μｍ程度の薄膜である場合には、事実上剥離は不可能であった。 For example, in the process of manufacturing individual semiconductor chips by dicing a semiconductor wafer, an adhesive tape called a dicing tape is attached to the semiconductor wafer for the purpose of protecting the semiconductor wafer from damage or the like ( For example, Patent Document 1). In the process of sticking the dicing tape to the semiconductor wafer, the sticking is usually performed by reducing the pressure so as not to cause air jamming. However, in this case, the dicing tape may be twisted by mistake. Poor wear may occur. If dicing is performed with the dicing tape twisted and stuck in this way, it is not only difficult to perform accurate dicing but also the semiconductor wafer may be damaged. Therefore, it is desirable to peel off the twisted dicing tape from the semiconductor wafer and reattach it. However, when trying to peel off the dicing tape, the semiconductor wafer may be damaged. In particular, in the case where the semiconductor wafer is a thin film having a thickness of about 50 μm, the separation was virtually impossible.
粘着テープの貼り直しを容易にするためには、例えば、粘着力を低く設定することが考えられる。しかしながら、上述のダイシングテープ等の用途では、ダイシング時の衝撃に耐えるためには、充分な粘着力が要求されており、粘着力を低く設定するにも限界がある。
貼着直後の初期粘着力が小さい一方で、その後に充分に高い粘着力を発揮することができる粘着テープが求められていた。
There has been a demand for an adhesive tape that can exhibit a sufficiently high adhesive force after the initial adhesive force is small immediately after sticking.
本発明は、貼着不良が発生した際に容易に剥離して貼り直すことが可能な粘着テープを提供することを目的とする。 An object of the present invention is to provide an adhesive tape that can be easily peeled off and reattached when a sticking failure occurs.
本発明は、貼着不良が発生した際に容易に剥離して貼り直すことが可能な粘着テープであって、基材の少なくとも一方の面に粘着剤層を有するものであり、前記粘着剤層は、ガラス転移温度が０〜１５℃である樹脂からなり、かつ、ゲル分率が４０〜７０％である貼り直しが容易な粘着テープである。
以下に本発明を詳述する。
The present invention is a pressure-sensitive adhesive tape that can be easily peeled off and reattached when a sticking failure occurs, and has a pressure-sensitive adhesive layer on at least one surface of the substrate. Is a pressure-sensitive adhesive tape made of a resin having a glass transition temperature of 0 to 15 ° C. and having a gel fraction of 40 to 70% and easy to reattach.
The present invention is described in detail below.
本発明者らは、粘着テープの粘着剤層を、ガラス転移温度が一定範囲である樹脂からなり、かつ、ゲル分率が一定範囲になるように調整することにより、貼着直後の初期粘着力は充分に小さく、容易に剥離して貼り直しができる一方、貼着後に時間が経過するに従って粘着力が向上する粘着テープが得られることを見出し、本発明を完成した。 By adjusting the pressure-sensitive adhesive layer of the pressure-sensitive adhesive tape made of a resin having a glass transition temperature in a certain range and a gel fraction within a certain range, the initial pressure-sensitive adhesive force immediately after sticking Was sufficiently small and could be easily peeled off and reattached, and on the other hand, it was found that an adhesive tape with improved adhesive strength was obtained as time passed, and the present invention was completed.
本発明の貼り直しが容易な粘着テープ（以下、単に「粘着テープ」ともいう。）は、基材の少なくとも一方の面に粘着剤層を有するものである。
本発明の粘着テープは、一方の面にのみ粘着剤層が形成された片面粘着テープであってもよく、両面に粘着剤層が形成された両面粘着テープであってもよい。
The pressure-sensitive adhesive tape (hereinafter also simply referred to as “pressure-sensitive adhesive tape”) that can be easily reattached according to the present invention has a pressure-sensitive adhesive layer on at least one surface of a substrate.
The pressure-sensitive adhesive tape of the present invention may be a single-sided pressure-sensitive adhesive tape in which a pressure-sensitive adhesive layer is formed only on one side, or may be a double-sided pressure-sensitive adhesive tape in which a pressure-sensitive adhesive layer is formed on both sides.
上記基材としては特に限定されず、例えば、アクリル、オレフィン、ポリカーボネート、塩化ビニル、ＡＢＳ、ポリエチレンテレフタレート（ＰＥＴ）、ナイロン、ウレタン、ポリイミド等の透明な樹脂からなるシート、網目状の構造を有するシート、孔が開けられたシート等が挙げられる。 The substrate is not particularly limited. For example, a sheet made of a transparent resin such as acrylic, olefin, polycarbonate, vinyl chloride, ABS, polyethylene terephthalate (PET), nylon, urethane, polyimide, or a sheet having a network structure. And a sheet having a hole formed therein.
上記粘着剤層を構成する樹脂は、ガラス転移温度の下限が０℃、上限が１５℃である。樹脂のガラス転移温度が０℃未満であると、貼着直後の初期粘着力が高くなり剥離が困難となり、１５℃を超えると、貼着後に時間が経過しても充分な粘着力を発揮できない。樹脂のガラス転移温度の好ましい下限は２℃、好ましい上限は１０℃である。
なお、２種以上の樹脂を併用したり、樹脂として共重合体を用いる場合には、該樹脂混合物や共重合体のガラス転移温度が上記範囲に調整されていれば同様の性能が得られる。
As for resin which comprises the said adhesive layer, the minimum of glass transition temperature is 0 degreeC, and an upper limit is 15 degreeC. If the glass transition temperature of the resin is less than 0 ° C., the initial adhesive strength immediately after pasting becomes high and peeling becomes difficult, and if it exceeds 15 ° C., sufficient adhesive strength cannot be exhibited even if time passes after pasting. . The minimum with a preferable glass transition temperature of resin is 2 degreeC, and a preferable upper limit is 10 degreeC.
In addition, when using 2 or more types of resin together, or using a copolymer as resin, if the glass transition temperature of this resin mixture or copolymer is adjusted to the said range, the same performance will be acquired.
上記粘着剤層を形成する樹脂としては特に限定されないが、例えば、（メタ）アクリル系モノマーを共重合してなる（メタ）アクリル系共重合体が好適である。
上記（メタ）アクリル系モノマーとしては特に限定されず、例えば、アルキル基の炭素数が２〜１８であるアクリル酸アルキルエステル、アルキル基の炭素数が２〜１８であるメタクリル酸アルキルエステル等が挙げられる。これらの（メタ）アクリル系モノマーは単独で用いてもよく、２種以上を併用してもよい。なかでも、メチルメタクリレートやアクリルニトリル等を主成分として用いることにより、得られる（メタ）アクリル系共重合体のガラス転移温度を容易に所期の範囲に調整することができる。
Although it does not specifically limit as resin which forms the said adhesive layer, For example, the (meth) acrylic-type copolymer formed by copolymerizing a (meth) acrylic-type monomer is suitable.
It does not specifically limit as said (meth) acrylic-type monomer, For example, the alkyl acrylate ester whose carbon number of an alkyl group is 2-18, the methacrylic acid alkyl ester whose carbon number of an alkyl group is 2-18, etc. are mentioned. It is done. These (meth) acrylic monomers may be used alone or in combination of two or more. Especially, the glass transition temperature of the (meth) acrylic-type copolymer obtained can be easily adjusted to the expected range by using methyl methacrylate, acrylonitrile, etc. as a main component.
上記（メタ）アクリル系モノマーとしては、ゲル分率を調整するために、２−ヒドロキシエチルアクリレート等の水酸基を有するモノマーや、アクリル酸等のカルボキシル基を有する極性モノマーを含有することが好ましい。 As said (meth) acrylic-type monomer, in order to adjust a gel fraction, it is preferable to contain the monomer which has hydroxyl groups, such as 2-hydroxyethyl acrylate, and the polar monomer which has carboxyl groups, such as acrylic acid.
上記粘着剤層は、光硬化性を有してもよい。光硬化型粘着剤からなる粘着剤層は、使用後に光の照射により粘着剤層の全体が均一にかつ速やかに重合架橋して一体化するため、重合硬化による弾性率の上昇が著しくなり、粘着力が大きく低下して剥離を行うことができる。 The pressure-sensitive adhesive layer may have photocurability. The pressure-sensitive adhesive layer made of a photo-curable pressure-sensitive adhesive is uniformly and quickly polymerized and cross-linked by light irradiation after use, so that the elastic modulus increases significantly due to polymerization and curing. The force is greatly reduced, and peeling can be performed.
上記粘着剤層に光硬化性を付与する方法としては特に限定されず、例えば、上記（メタ）アクリル系共重合体として分子内にラジカル重合性の不飽和結合を有する重合性ポリマーを用い、更に、ラジカル重合性の多官能オリゴマー又はモノマー、及び、光重合開始剤を配合する方法が挙げられる。 The method for imparting photocurability to the pressure-sensitive adhesive layer is not particularly limited. For example, a polymerizable polymer having a radical polymerizable unsaturated bond in the molecule is used as the (meth) acrylic copolymer. , Radical polymerizable polyfunctional oligomer or monomer, and a method of blending a photopolymerization initiator.
上記粘着剤層は、ゲル分率の下限が４０％、上限が７０％である。ゲル分率が４０％未満であると、貼着直後の初期粘着力が高くなり剥離が困難となり、７０％を超えると、貼着後に時間が経過しても充分な粘着力を発揮できない。ゲル分率の好ましい下限は５０％、好ましい上限は６５％である。
なお、上記ゲル分率は、以下の方法により測定することができる。
上記粘着剤層の重量Ｗ１を測定する。これを酢酸エチル中に２３℃にて２４時間浸漬した後、２００メッシュのステンレスメッシュを介して試験片を酢酸エチルから取り出して、１１０℃の条件下で１時間乾燥させる。そして、乾燥後の試験片の重量Ｗ２を測定し、下記式を用いてゲル分率を算出する。
ゲル分率（重量％）＝１００×Ｗ２／Ｗ１
The adhesive layer has a gel fraction lower limit of 40% and an upper limit of 70%. If the gel fraction is less than 40%, the initial adhesive force immediately after sticking becomes high and peeling becomes difficult, and if it exceeds 70%, sufficient adhesive force cannot be exhibited even if time passes after sticking. The preferable lower limit of the gel fraction is 50%, and the preferable upper limit is 65%.
In addition, the said gel fraction can be measured with the following method.
The weight W 1 of the pressure-sensitive adhesive layer is measured. After immersing this in ethyl acetate at 23 ° C. for 24 hours, the test piece is taken out from the ethyl acetate through a 200-mesh stainless mesh and dried at 110 ° C. for 1 hour. Then, the weight W 2 after drying the test piece was measured to calculate the gel fraction using the following equation.
Gel fraction (% by weight) = 100 × W 2 / W 1
上記粘着剤層のゲル分率を調整する方法としては、例えば、架橋剤の添加量を調整する方法が挙げられる。
上記架橋剤としては特に限定されず、例えば、イソシアネート系架橋剤、アジリジン系架橋剤、エポキシ系架橋剤、金属キレート型架橋剤等が挙げられる。これらの架橋剤は、単独で用いてもよく、２種以上を併用してもよい。
Examples of the method for adjusting the gel fraction of the pressure-sensitive adhesive layer include a method for adjusting the addition amount of the crosslinking agent.
It does not specifically limit as said crosslinking agent, For example, an isocyanate type crosslinking agent, an aziridine type crosslinking agent, an epoxy-type crosslinking agent, a metal chelate type crosslinking agent etc. are mentioned. These crosslinking agents may be used independently and may use 2 or more types together.
本発明の粘着テープは、貼着直後の初期粘着力は充分に小さく、容易に剥離して貼り直しができる一方、貼着後に時間が経過するに従って粘着力が向上するという性能を発揮する。この理由については明らかではないが、以下のように推測される。
そもそも、ガラス転移温度が０〜１５℃である樹脂からなり、かつ、ゲル分率が４０〜７０％である粘着剤層は、粘着力が低く、通常では粘着テープに用いられることはない。このため、貼着直後にはほとんど粘着力がなく、容易に貼り直しができる。しかしながら、被着体が平滑面である場合には、貼着後に時間が経過するに従って粘着力が向上する。これは、粘着剤の流動成分（ゾル分）が時間とともに流動し、被着体表面に濡れていき、接着面積を増大させるためであると考えられる。
The pressure-sensitive adhesive tape of the present invention has a sufficiently low initial pressure-sensitive adhesive force immediately after sticking, and can be easily peeled off and re-sticked, while exhibiting the performance of improving the pressure-sensitive adhesive force as time passes after sticking. The reason for this is not clear, but is presumed as follows.
In the first place, the pressure-sensitive adhesive layer made of a resin having a glass transition temperature of 0 to 15 ° C. and having a gel fraction of 40 to 70% has low adhesive force and is not usually used for a pressure-sensitive adhesive tape. For this reason, there is almost no adhesive force immediately after sticking, and it can be easily stuck again. However, when the adherend is a smooth surface, the adhesive force improves as time passes after sticking. This is presumably because the flow component (sol content) of the pressure-sensitive adhesive flows with time, wets the adherend surface, and increases the adhesion area.
常温（２３℃程度）で貼着を行う場合、上記範囲のガラス転移温度を有する樹脂はその流動性が小さいことから、被着体の表面が大きな凹凸を有する粗面であると接着面積を有効に拡大させることは難しい。従って、本発明の粘着テープが適用可能な被着体は平滑面を有するものに限られる。最終的に要求される粘着力にもよるが、本発明の粘着テープが適用等被着体としては、表面の粗さが３μｍ以下であるもの、好ましくは１μｍ以下であるものとなる。この程度の平滑面を有するものであれば、シリコンウエハ、ガラス、金属等のいずれであっても本発明の効果を得ることができる。 When pasting at room temperature (about 23 ° C), the resin having a glass transition temperature in the above range has a low fluidity, so that the surface of the adherend is a rough surface having large irregularities, which makes the bonding area effective. It is difficult to expand. Therefore, the adherend to which the adhesive tape of the present invention can be applied is limited to one having a smooth surface. Although it depends on the finally required adhesive strength, the adherend to which the adhesive tape of the present invention is applied has a surface roughness of 3 μm or less, preferably 1 μm or less. As long as it has such a smooth surface, the effect of the present invention can be obtained with any of silicon wafer, glass, metal and the like.
本発明によれば、貼着不良が発生した際に容易に剥離して貼り直すことが可能な粘着テープを提供することができる。 According to the present invention, it is possible to provide an adhesive tape that can be easily peeled off and reattached when a sticking failure occurs.
以下に実施例を挙げて本発明の態様を更に詳しく説明するが、本発明はこれら実施例にのみ限定されるものではない。 Hereinafter, embodiments of the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.
（実験例１）
（１）下記の化合物を酢酸エチルに溶解させ、紫外線を照射して重合を行い、重量平均分子量４０万のアクリル共重合体からなる粘着剤の酢酸エチル溶液を得た。
エチルアクリレート ８０重量部
２−ヒドロキシエチルメタクリレート ５重量部
アクリル酸 ５重量部
アクリロニトリル ９重量部
光重合開始剤 １重量部
（イルガキュア６５１、５０％酢酸エチル溶液）
ラウリルメルカプタン ０．５重量部
得られたアクリル共重合体について、動的粘弾性測定ＤＶＡ−２００（アイティー計測制御社製）を用いて、剪断弾性率、歪５％、周波数１０Ｈｚの条件にてガラス転移温度を測定したところ、−５℃であった。
(Experimental example 1)
(1) The following compounds were dissolved in ethyl acetate and polymerized by irradiating with ultraviolet rays to obtain an ethyl acetate solution of an adhesive composed of an acrylic copolymer having a weight average molecular weight of 400,000.
Ethyl acrylate 80 parts by weight 2-hydroxyethyl methacrylate 5 parts by weight Acrylic acid 5 parts by weight Acrylonitrile 9 parts by weight Photopolymerization initiator 1 part by weight (Irgacure 651, 50% ethyl acetate solution)
About 0.5 parts by weight of lauryl mercaptan The obtained acrylic copolymer was subjected to dynamic viscoelasticity measurement DVA-200 (manufactured by IT Measurement & Control Co., Ltd.) under conditions of shear elastic modulus, strain 5%, frequency 10 Hz. It was -5 degreeC when the glass transition temperature was measured.
（２）粘着剤層用組成物溶液の調製
得られた粘着剤の酢酸エチル溶液の樹脂固形分１００重量部に対して、２−イソシアナトエチルメタクリレートを加えて反応させた。この際、形成される粘着剤層のゲル分率が３５、４０、５５、７０、７５％となるように、２−イソシアナトエチルメタクリレートの配合量の異なる５種類の粘着剤層用組成物溶液を調製した。
(2) Preparation of composition solution for pressure-sensitive adhesive layer 2-isocyanatoethyl methacrylate was added and reacted with respect to 100 parts by weight of resin solid content of the obtained pressure-sensitive adhesive in ethyl acetate solution. Under the present circumstances, the composition solution for five types of adhesive layers from which the compounding quantity of 2-isocyanatoethyl methacrylate differs so that the gel fraction of the adhesive layer formed may be 35, 40, 55, 70, 75%. Was prepared.
（３）粘着テープの製造
得られた粘着剤層用組成物溶液を、片面にコロナ処理を施した厚さ７５μｍの透明なポリエチレンテレフタレート（ＰＥＴ）フィルムのコロナ処理上に乾燥皮膜の厚さが約１５μｍとなるようにドクターナイフで塗工し１１０℃、５分間加熱して塗工溶液を乾燥させた。次いで、粘着剤層の表面に離型処理が施されたＰＥＴフィルムを貼り付けた。その後、４０℃、３日間静置養生を行い、粘着テープを得た。
(3) Manufacture of pressure-sensitive adhesive tape The obtained composition solution for pressure-sensitive adhesive layer was subjected to a corona treatment on a transparent polyethylene terephthalate (PET) film having a thickness of 75 μm with one side subjected to a corona treatment. Coating was performed with a doctor knife so as to be 15 μm, and the coating solution was dried by heating at 110 ° C. for 5 minutes. Next, a PET film that was subjected to a release treatment was attached to the surface of the pressure-sensitive adhesive layer. Thereafter, static curing was performed at 40 ° C. for 3 days to obtain an adhesive tape.
（実験例２）
（１）下記の化合物を酢酸エチルに溶解させ、紫外線を照射して重合を行い、重量平均分子量４５万のアクリル共重合体からなる粘着剤の酢酸エチル溶液を得た。
エチルアクリレート ７０重量部
２−ヒドロキシエチルメタクリレート ３重量部
メチルメタクリレート ２７重量部
光重合開始剤 １重量部
（イルガキュア６５１、５０％酢酸エチル溶液）
ラウリルメルカプタン ０．５重量部
得られたアクリル共重合体について、実験例１と同様の方法によりガラス転移温度を測定したところ、０℃であった。
(Experimental example 2)
(1) The following compound was dissolved in ethyl acetate and polymerized by irradiating with ultraviolet rays to obtain an ethyl acetate solution of an adhesive made of an acrylic copolymer having a weight average molecular weight of 450,000.
Ethyl acrylate 70 parts by weight 2-hydroxyethyl methacrylate 3 parts by weight methyl methacrylate 27 parts by weight Photopolymerization initiator 1 part by weight (Irgacure 651, 50% ethyl acetate solution)
About 0.5 parts by weight of lauryl mercaptan, the obtained acrylic copolymer was measured for glass transition temperature by the same method as in Experimental Example 1 and found to be 0 ° C.
（２）粘着剤層用組成物溶液の調製
得られた粘着剤の酢酸エチル溶液の樹脂固形分１００重量部に対して、２−イソシアナトエチルメタクリレートを加えて反応させた。この際、形成される粘着剤層のゲル分率が３５、４０、５５、７０、７５％となるように、２−イソシアナトエチルメタクリレートの配合量の異なる５種類の粘着剤層用組成物溶液を調製した。
(2) Preparation of composition solution for pressure-sensitive adhesive layer 2-isocyanatoethyl methacrylate was added and reacted with respect to 100 parts by weight of resin solid content of the obtained pressure-sensitive adhesive in ethyl acetate solution. Under the present circumstances, the composition solution for five types of adhesive layers from which the compounding quantity of 2-isocyanatoethyl methacrylate differs so that the gel fraction of the adhesive layer formed may be 35, 40, 55, 70, 75%. Was prepared.
（３）粘着テープの製造
得られた粘着剤層用組成物溶液を、片面にコロナ処理を施した厚さ７５μｍの透明なポリエチレンテレフタレート（ＰＥＴ）フィルムのコロナ処理上に乾燥皮膜の厚さが約１５μｍとなるようにドクターナイフで塗工し１１０℃、５分間加熱して塗工溶液を乾燥させた。次いで、粘着剤層の表面に離型処理が施されたＰＥＴフィルムを貼り付けた。その後、４０℃、３日間静置養生を行い、粘着テープを得た。
(3) Manufacture of pressure-sensitive adhesive tape The obtained composition solution for pressure-sensitive adhesive layer was subjected to a corona treatment on a transparent polyethylene terephthalate (PET) film having a thickness of 75 μm with one side subjected to a corona treatment. Coating was performed with a doctor knife so as to be 15 μm, and the coating solution was dried by heating at 110 ° C. for 5 minutes. Next, a PET film that was subjected to a release treatment was attached to the surface of the pressure-sensitive adhesive layer. Thereafter, static curing was performed at 40 ° C. for 3 days to obtain an adhesive tape.
（実験例３）
（１）下記の化合物を酢酸エチルに溶解させ、紫外線を照射して重合を行い、重量平均分子量４３万のアクリル共重合体からなる粘着剤の酢酸エチル溶液を得た。
エチルアクリレート ６５重量部
２−ヒドロキシエチルメタクリレート ３重量部
メチルメタクリレート ３２重量部
光重合開始剤 １重量部
（イルガキュア６５１、５０％酢酸エチル溶液）
ラウリルメルカプタン ０．５重量部
得られたアクリル共重合体について、実験例１と同様の方法によりガラス転移温度を測定したところ、１０℃であった。
(Experimental example 3)
(1) The following compound was dissolved in ethyl acetate and polymerized by irradiating with ultraviolet rays to obtain an ethyl acetate solution of an adhesive made of an acrylic copolymer having a weight average molecular weight of 430,000.
Ethyl acrylate 65 parts by weight 2-hydroxyethyl methacrylate 3 parts by weight methyl methacrylate 32 parts by weight Photopolymerization initiator 1 part by weight (Irgacure 651, 50% ethyl acetate solution)
About 0.5 parts by weight of lauryl mercaptan, the obtained acrylic copolymer was measured for glass transition temperature by the same method as in Experimental Example 1 and found to be 10 ° C.
（２）粘着剤層用組成物溶液の調製
得られた粘着剤の酢酸エチル溶液の樹脂固形分１００重量部に対して、２−イソシアナトエチルメタクリレートを加えて反応させた。この際、形成される粘着剤層のゲル分率が３５、４０、５５、７０、７５％となるように、２−イソシアナトエチルメタクリレートの配合量の異なる５種類の粘着剤層用組成物溶液を調製した。
(2) Preparation of composition solution for pressure-sensitive adhesive layer 2-isocyanatoethyl methacrylate was added and reacted with respect to 100 parts by weight of resin solid content of the obtained pressure-sensitive adhesive in ethyl acetate solution. Under the present circumstances, the composition solution for five types of adhesive layers from which the compounding quantity of 2-isocyanatoethyl methacrylate differs so that the gel fraction of the adhesive layer formed may be 35, 40, 55, 70, 75%. Was prepared.
（３）粘着テープの製造
得られた粘着剤層用組成物溶液を、片面にコロナ処理を施した厚さ７５μｍの透明なポリエチレンテレフタレート（ＰＥＴ）フィルムのコロナ処理上に乾燥皮膜の厚さが約１５μｍとなるようにドクターナイフで塗工し１１０℃、５分間加熱して塗工溶液を乾燥させた。次いで、粘着剤層の表面に離型処理が施されたＰＥＴフィルムを貼り付けた。その後、４０℃、３日間静置養生を行い、粘着テープを得た。
(3) Manufacture of pressure-sensitive adhesive tape The obtained composition solution for pressure-sensitive adhesive layer was subjected to a corona treatment on a transparent polyethylene terephthalate (PET) film having a thickness of 75 μm with one side subjected to a corona treatment. Coating was performed with a doctor knife so as to be 15 μm, and the coating solution was dried by heating at 110 ° C. for 5 minutes. Next, a PET film that was subjected to a release treatment was attached to the surface of the pressure-sensitive adhesive layer. Thereafter, static curing was performed at 40 ° C. for 3 days to obtain an adhesive tape.
（実験例４）
（１）下記の化合物を酢酸エチルに溶解させ、紫外線を照射して重合を行い、重量平均分子量４８万のアクリル共重合体からなる粘着剤の酢酸エチル溶液を得た。
エチルアクリレート ６０重量部
２−ヒドロキシエチルメタクリレート ３重量部
メチルメタクリレート ３７重量部
光重合開始剤 １重量部
（イルガキュア６５１、５０％酢酸エチル溶液）
ラウリルメルカプタン ０．５重量部
得られたアクリル共重合体について、実験例１と同様の方法によりガラス転移温度を測定したところ、１５℃であった。
(Experimental example 4)
(1) The following compound was dissolved in ethyl acetate and polymerized by irradiating with ultraviolet rays to obtain an ethyl acetate solution of a pressure-sensitive adhesive made of an acrylic copolymer having a weight average molecular weight of 480,000.
Ethyl acrylate 60 parts by weight 2-hydroxyethyl methacrylate 3 parts by weight methyl methacrylate 37 parts by weight Photopolymerization initiator 1 part by weight (Irgacure 651, 50% ethyl acetate solution)
About 0.5 parts by weight of lauryl mercaptan, the obtained acrylic copolymer was measured for glass transition temperature by the same method as in Experimental Example 1 and found to be 15 ° C.
（２）粘着剤層用組成物溶液の調製
得られた粘着剤の酢酸エチル溶液の樹脂固形分１００重量部に対して、２−イソシアナトエチルメタクリレートを加えて反応させた。この際、形成される粘着剤層のゲル分率が３５、４０、５５、７０、７５％となるように、２−イソシアナトエチルメタクリレートの配合量の異なる５種類の粘着剤層用組成物溶液を調製した。
(2) Preparation of composition solution for pressure-sensitive adhesive layer 2-isocyanatoethyl methacrylate was added and reacted with respect to 100 parts by weight of resin solid content of the obtained pressure-sensitive adhesive in ethyl acetate solution. Under the present circumstances, the composition solution for five types of adhesive layers from which the compounding quantity of 2-isocyanatoethyl methacrylate differs so that the gel fraction of the adhesive layer formed may be 35, 40, 55, 70, 75%. Was prepared.
（３）粘着テープの製造
得られた粘着剤層用組成物溶液を、片面にコロナ処理を施した厚さ７５μｍの透明なポリエチレンテレフタレート（ＰＥＴ）フィルムのコロナ処理上に乾燥皮膜の厚さが約１５μｍとなるようにドクターナイフで塗工し１１０℃、５分間加熱して塗工溶液を乾燥させた。次いで、粘着剤層の表面に離型処理が施されたＰＥＴフィルムを貼り付けた。その後、４０℃、３日間静置養生を行い、粘着テープを得た。
(3) Manufacture of pressure-sensitive adhesive tape The obtained composition solution for pressure-sensitive adhesive layer was subjected to a corona treatment on a transparent polyethylene terephthalate (PET) film having a thickness of 75 μm with one side subjected to a corona treatment. Coating was performed with a doctor knife so as to be 15 μm, and the coating solution was dried by heating at 110 ° C. for 5 minutes. Next, a PET film that was subjected to a release treatment was attached to the surface of the pressure-sensitive adhesive layer. Thereafter, static curing was performed at 40 ° C. for 3 days to obtain an adhesive tape.
（実験例５）
（１）下記の化合物を酢酸エチルに溶解させ、紫外線を照射して重合を行い、重量平均分子量４０万のアクリル共重合体からなる粘着剤の酢酸エチル溶液を得た。
エチルアクリレート ５６重量部
２−ヒドロキシエチルメタクリレート ４重量部
メチルメタクリレート ３５重量部
アクリロニトリル ５重量部
光重合開始剤 １重量部
（イルガキュア６５１、５０％酢酸エチル溶液）
ラウリルメルカプタン ０．５重量部
得られたアクリル共重合体について、実験例１と同様の方法によりガラス転移温度を測定したところ、２０℃であった。
(Experimental example 5)
(1) The following compounds were dissolved in ethyl acetate and polymerized by irradiating with ultraviolet rays to obtain an ethyl acetate solution of an adhesive composed of an acrylic copolymer having a weight average molecular weight of 400,000.
Ethyl acrylate 56 parts by weight 2-hydroxyethyl methacrylate 4 parts by weight Methyl methacrylate 35 parts by weight Acrylonitrile 5 parts by weight Photopolymerization initiator 1 part by weight (Irgacure 651, 50% ethyl acetate solution)
About 0.5 parts by weight of lauryl mercaptan, the obtained acrylic copolymer was measured for glass transition temperature by the same method as in Experimental Example 1 and found to be 20 ° C.
（２）粘着剤層用組成物溶液の調製
得られた粘着剤の酢酸エチル溶液の樹脂固形分１００重量部に対して、２−イソシアナトエチルメタクリレートを加えて反応させた。この際、形成される粘着剤層のゲル分率が３５、４０、５５、７０、７５％となるように、２−イソシアナトエチルメタクリレートの配合量の異なる５種類の粘着剤層用組成物溶液を調製した。
(2) Preparation of composition solution for pressure-sensitive adhesive layer 2-isocyanatoethyl methacrylate was added and reacted with respect to 100 parts by weight of resin solid content of the obtained pressure-sensitive adhesive in ethyl acetate solution. Under the present circumstances, the composition solution for five types of adhesive layers from which the compounding quantity of 2-isocyanatoethyl methacrylate differs so that the gel fraction of the adhesive layer formed may be 35, 40, 55, 70, 75%. Was prepared.
（３）粘着テープの製造
得られた粘着剤層用組成物溶液を、片面にコロナ処理を施した厚さ７５μｍの透明なポリエチレンテレフタレート（ＰＥＴ）フィルムのコロナ処理上に乾燥皮膜の厚さが約１５μｍとなるようにドクターナイフで塗工し１１０℃、５分間加熱して塗工溶液を乾燥させた。次いで、粘着剤層の表面に離型処理が施されたＰＥＴフィルムを貼り付けた。その後、４０℃、３日間静置養生を行い、粘着テープを得た。
(3) Manufacture of pressure-sensitive adhesive tape The obtained composition solution for pressure-sensitive adhesive layer was subjected to a corona treatment on a transparent polyethylene terephthalate (PET) film having a thickness of 75 μm with one side subjected to a corona treatment. Coating was performed with a doctor knife so as to be 15 μm, and the coating solution was dried by heating at 110 ° C. for 5 minutes. Next, a PET film that was subjected to a release treatment was attached to the surface of the pressure-sensitive adhesive layer. Thereafter, static curing was performed at 40 ° C. for 3 days to obtain an adhesive tape.
（評価）
実験例１〜５で製造した、樹脂のガラス転移温度とゲル分率とが異なる２５種類の粘着テープについて、以下のように評価を行った。
結果を表１に示した。
(Evaluation)
The 25 types of pressure-sensitive adhesive tapes produced in Experimental Examples 1 to 5 having different glass transition temperatures and different gel fractions were evaluated as follows.
The results are shown in Table 1.
（１）貼着直後の剥離力の測定
被着体として、表面の粗さが０．５μｍ以下であるシリコンミラーウエハを準備した。得られた粘着テープを２５ｍｍ幅×１００ｍｍ長さにカットしたサンプルから離型処理が施されたＰＥＴフィルムを剥離し、その粘着剤層面を上記シリコンウエハ上に重ね合わせて２ｋｇのローラで１往復押圧し、粘着テープをシリコンウエハ上に貼着した。
(1) Measurement of peeling force immediately after sticking A silicon mirror wafer having a surface roughness of 0.5 μm or less was prepared as an adherend. The PET film that has been subjected to the release treatment is peeled off from the sample obtained by cutting the obtained adhesive tape into a width of 25 mm and a length of 100 mm, and the pressure-sensitive adhesive layer surface is superimposed on the silicon wafer and pressed once with a 2 kg roller. Then, an adhesive tape was stuck on the silicon wafer.
貼着直後に、ＪＩＳ Ｋ ６８５４に準拠した１８０°ピール剥離力を測定した。剥離測定速度は３００ｍｍ／ｍｉｎとした。 Immediately after sticking, 180 ° peel peel strength in accordance with JIS K 6854 was measured. The peel measurement speed was 300 mm / min.
（２）貼着３０分後の剥離力の測定
（１）と同様の方法により粘着テープをシリコンウエハ上に貼着した後、２３℃の温度条件下、３０分間放置した。その後、ＪＩＳ Ｋ ６８５４に準拠した１８０°ピール剥離力を測定した。剥離測定速度は３００ｍｍ／ｍｉｎとした。
(2) Measurement of peel force after 30 minutes of sticking The adhesive tape was stuck on a silicon wafer by the same method as in (1), and then left for 30 minutes at a temperature of 23 ° C. Thereafter, 180 ° peel peel strength in accordance with JIS K 6854 was measured. The peel measurement speed was 300 mm / min.
（３）全体評価
得られた貼着直後の剥離力及び貼着３０分後の剥離力より、貼着直後の剥離力が１Ｎ／２５ｍｍ以下であり、かつ、貼着３０分後の剥離力が８Ｎ／２５ｍｍ以上である場合を「○」と、貼着直後の剥離力が１Ｎ／２５ｍｍ以下であるが、貼着３０分後の剥離力が８Ｎ／２５ｍｍ未満である場合を「△」と、貼着直後の剥離力が１Ｎ／２５ｍｍを超えるが、貼着３０分後の剥離力が８Ｎ／２５ｍｍ以上である場合を「▲」と、貼着直後の剥離力が１Ｎ／２５ｍｍを超え、かつ、貼着３０分後の剥離力が８Ｎ／２５ｍｍ未満である場合を「×」と評価した。
なお、剥離力が１Ｎ／２５ｍｍを超えると剥離が困難であり、また、剥離力が８Ｎ／２５ｍｍ未満であるとダイシングテープとしては使用困難であることから、基準を設定した。
(3) Overall evaluation From the obtained peel force immediately after sticking and peel force after 30 minutes of sticking, the peel force immediately after sticking is 1 N / 25 mm or less, and the peel force after 30 minutes of sticking is The case where it is 8 N / 25 mm or more is “◯”, and the peel force immediately after sticking is 1 N / 25 mm or less, but the case where the peel force after 30 minutes of sticking is less than 8 N / 25 mm is “△”, The peel force immediately after sticking exceeds 1 N / 25 mm, but when the peel force after 30 minutes of sticking is 8 N / 25 mm or more, “▲”, the peel force immediately after sticking exceeds 1 N / 25 mm, and The case where the peel force after 30 minutes of attachment was less than 8 N / 25 mm was evaluated as “x”.
In addition, since peeling was difficult when peeling force exceeded 1 N / 25mm and it was difficult to use as a dicing tape when peeling force was less than 8 N / 25mm, the reference | standard was set.
本発明によれば、貼着不良が発生した際に容易に剥離して貼り直すことが可能な粘着テープを提供することができる。
According to the present invention, it is possible to provide an adhesive tape that can be easily peeled off and reattached when a sticking failure occurs.
Claims (1)
基材の少なくとも一方の面に粘着剤層を有するものであり、
前記粘着剤層は、ガラス転移温度が０〜１５℃である樹脂からなり、かつ、ゲル分率が４０〜７０％である
ことを特徴とする貼り直しが容易な粘着テープ。
It is an adhesive tape that can be easily peeled off and reattached when a sticking failure occurs,
It has an adhesive layer on at least one surface of the substrate,
The pressure-sensitive adhesive layer is made of a resin having a glass transition temperature of 0 to 15 ° C., and has a gel fraction of 40 to 70%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015073056A (en) * | 2013-10-04 | 2015-04-16 | リンテック株式会社 | Sheet for semiconductor processing |
| JP2015126082A (en) * | 2013-12-26 | 2015-07-06 | 株式会社デンソー | Semiconductor chip pickup method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10306267A (en) * | 1997-05-08 | 1998-11-17 | Sekisui Chem Co Ltd | Autohesive sheet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10306267A (en) * | 1997-05-08 | 1998-11-17 | Sekisui Chem Co Ltd | Autohesive sheet |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015073056A (en) * | 2013-10-04 | 2015-04-16 | リンテック株式会社 | Sheet for semiconductor processing |
| JP2015126082A (en) * | 2013-12-26 | 2015-07-06 | 株式会社デンソー | Semiconductor chip pickup method |
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